食品科学 ›› 2019, Vol. 40 ›› Issue (16): 335-342.doi: 10.7506/spkx1002-6630-20190107-097

• 安全检测 • 上一篇    下一篇

TLC-UPLC-MS/MS法检测网红保健品中非法添加的8种化学药物

曹晓琴,方振峰,张 涛,周国勇,陈中强,施 璐   

  1. 江汉大学医学院,湖北 武汉 430056
  • 出版日期:2019-08-25 发布日期:2019-08-26
  • 基金资助:
    江汉大学高层次人才科研启动项目(08250001)

Determination of Eight Illegal Drugs in Internet-Famous Health Foods by Thin-Layer Chromatography Coupled to Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

CAO Xiaoqin, FANG Zhenfeng, ZHANG Tao, ZHOU Guoyong, CHEN Zhongqiang, SHI Lu   

  1. College of Medicine, Jianghan University, Wuhan 430056, China
  • Online:2019-08-25 Published:2019-08-26

摘要: 建立薄层色谱-超高效液相色谱-串联质谱法同时检测网红保健品中非法添加的8 种化学药物。样品采用薄层色谱法进行前处理,采用Kinetex 100 RP-18(100 mm×2.1 mm,1.6 μm)色谱柱分离,以乙腈-1 mmol/L乙酸铵(含0.1%乙酸)溶液为流动相梯度洗脱,采用多重反应监测方式检测西布曲明、洛伐他汀、辛伐他汀、麻黄碱、咖啡因、酚酞、苯乙双胍和西地那非等8 种药物。结果表明,8 种化合物在0.5~100 μg/L范围内线性关系良好,相关系数≥0.995 8,各组分的检出限在0.09~0.29 μg/kg之间,定量限在0.31~0.79 μg/kg之间。待测物在不同样品中的平均回收率介于67.3%~101.1%,变异系数≤16.5%。45 批保健食品检出23 批非法添加阳性样品。本法经方法学验证,可用于网红保健品中8 种非法添加药物的快速筛查和定量测定。

关键词: 薄层色谱, 超高效液相色谱-串联质谱, 网红保健品, 非法添加

Abstract: A method for the simultaneous determination of 8 illegal drugs in internet-famous health foods was established by thin-layer chromatography (TLC) coupled to ultra performance liquid chromatography-tandem mass spectrometry (TLC-UPLC-MS/MS). The sample pretreatment was accomplished by TLC, and subsequently the chromatographic separation was done on a Kinetex 100 RP-18 (100 mm × 2.1 mm, 1.6 μm) column with gradient elution using a mobile phase consisting of 1 mmol/L ammonium acetate solution (with 0.1% acetic acid) and acetonitrile. The multiple reaction monitoring (MRM) mode was used to quantify 8 illegal drugs, sibutramine, lovastatin, simvastatin, ephedrine, caffeine, phenolphthalein, phenformin and sildenafil. The results showed that good linear relationships in the range of 0.5–100 μg/L were observed for all of the analytes with correlation coefficients no less than 0.995 8. The limits of detection (LODs) and limits of quantification (LOQs) ranged from 0.09 to 0.29 μg/kg and from 0.31 to 0.79 μg/kg, respectively. The average recoveries for various samples were in the range of 67.3%–101.1%, and the relative standard deviations for six replicate determinations were no more than 16.5%. Totally, 23 out of 45 samples were identified to contain the illegal drugs. The established method can be suitable for rapid screening and quantification of these 8 illegal drugs in internet-famous health foods.

Key words: thin-layer chromatography, ultra performance liquid chromatography-tandem mass spectrometry, internetfamous health foods, illicit drugs

中图分类号: